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| United States Patent |
5,320,827
|
|
Conway
, et al.
|
June 14, 1994
|
Encapsulated aluminum-zirconium compositions
Abstract
Encapsulated aluminum-zirconium salt compositions are produced by combining
and heating an aqueous aluminum- zirconium salt selected from
aluminum-zirconium halohydrates and mixtures thereof; a hydrophobic
liquid; and a carboxylate. The mixture is heated until substantially all
of the free water has been removed. The encapsulated aluminum-zirconium
salts precipitate out after the removal of the water. The encapsulated
aluminum-zirconium salts are useful in deodorant and antiperspirant
compositions.
| Inventors:
|
Conway; Lori J. (Hope, MI);
Katsoulis; Dimitris E. (Midland, MI);
Schulz, Jr.; William J. (Midland, MI)
|
| Assignee:
|
Dow Corning Corporation (Midland, MI)
|
| Appl. No.:
|
073194 |
| Filed:
|
June 8, 1993 |
| Current U.S. Class: |
424/47; 424/66; 424/401; 424/DIG.5 |
| Intern'l Class: |
A61K 007/34; A61K 009/12 |
| Field of Search: |
424/47,DIG. 5,68
|
References Cited
U.S. Patent Documents
| 4524062 | Jun., 1985 | Laba et al. | 424/65.
|
| 4803195 | Feb., 1989 | Holzner | 512/4.
|
| 4818522 | Apr., 1989 | Ferentchak | 424/66.
|
| Foreign Patent Documents |
| 0303461 | Oct., 1988 | EP | .
|
| 6049285 | Oct., 1986 | JP | .
|
Other References
S. Cohen, et al.; J. Am. Chem. Soc. 1990; "Ionically Cross-Linkable
Polyphosphazene: A Novel Polymer for Microencapsulation"; 112, pp.
7832-7833.
R. Dagani; C&EN; "Polyphosphazene Encapsulates Living Cells"; Oct. 22,
1990, p. 28.
|
Primary Examiner: Ore; Dale R.
Attorney, Agent or Firm: Severance; Sharon K.
Parent Case Text
This is a divisional of copending application(s) Ser. No. 07/742,671 filed
on Aug. 7, 1991 which is a continuation-in-part of Ser. No. 07/631,308
both now abandoned.
Claims
What is claimed is:
1. An aerosol composition comprising
(A) 1% to 20% by weight of an encapsulated aluminum-zirconium salt
composition comprising
(I) an aluminum-zirconium salt selected from the group consisting of
aluminum-zirconium halohydrates; contained in a shell comprising
(II) a carboxylate or mixture of carboxylates selected from the group
consisting of carboxylates having the formula
##STR4##
wherein R.sup.1 is selected from the group consisting of a saturated or
unsaturated, branched or linear alkyl group consisting of at least 2
carbon atoms, a phenyl group, and a phenyl ethylene group; and Z is
selected from the group consisting of hydrogen atoms, alkali metals,
glyceryl and mixtures thereof;
(B) 50% to 90% by weight of propellant; and
(C) 5% to 15% by weight of an anhydrous carrier liquid.
2. The aerosol composition as claimed in claim 1 wherein the composition is
comprised of 8% to 12% by weight of the encapsulated aluminum-zirconium
salt.
3. A stick composition comprising
(A) 1% to 20% by weight of an encapsulated aluminum-zirconium salt
composition comprising
(I) an aluminum-zirconium salt selected from the group consisting of
aluminum-zirconium halohydrates; contained in a shell comprising
(II) a carboxylate or mixture of carboxylates selected from the group
consisting of carboxylates having the formula
##STR5##
wherein R.sup.1 is selected from the group consisting of a saturated or
unsaturated, branched or linear alkyl group consisting of at least 2
carbon atoms, a phenyl group, and a phenyl ethylene group; and Z is
selected from the group consisting of hydrogen atoms, alkali metals,
glyceryl and mixtures thereof;
(B) 20% to 65% by weight of a carrier fluid; and
(C) 5% to 30% by weight of a gellant.
4. A roll-on composition comprising
(A) 1% to 20% by weight of an encapsulated aluminum-zirconium salt
composition comprising
(I) an aluminum-zirconium salt selected from the group consisting of
aluminum-zirconium halohydrates; contained in a shell comprising
(II) a carboxylate or mixture of carboxylates selected from the group
consisting of carboxylates having the formula
##STR6##
wherein R.sup.1 is selected from the group consisting of a saturated or
unsaturated, branched or linear alkyl group consisting of at least 2
carbon atoms, a phenyl group, and a phenyl ethylene group; and Z is
selected from the group consisting of hydrogen atoms, alkali metals,
glyceryl and mixtures thereof; and
(B) 60% to 90% by weight of a carrier fluid.
Description
This invention pertains to encapsulated aluminum-zirconium halohydrate
compounds. An aluminum-zirconium halohydrate salt is encapsulated in a
shell comprising a carboxylate, such as stearic acid. The
aluminum-zirconium salts are released from the encapsulant in the presence
of moisture and are useful in antiperspirant and deodorant compositions.
BACKGROUND OF THE INVENTION
It is known in the art to coat or encapsulate certain materials to provide
a protective barrier to the material and/or to control the release
characteristic of the material. A coated material is typically surrounded
by a film wherein the film is "adhered" to the composition. An
encapsulated material is typically surrounded by a film in the form of a
shell or capsule wherein the shell or capsule is not necessarily adhered
to the composition.
Topically applied materials such as cosmetics, lotions, fragrances,
antiperspirants and deodorants, which contain ingredients that are
encapsulated or coated, are known in the art. For example, Japanese Patent
No. 86049285 teaches a transparent cosmetic composition comprising a fine
powdered mica which is coated with a mixture of a hydrocarbon, a fatty
acid, and a silicone oil and then baked at 100.degree. C. to 150.degree.
C. for 1 to 5 hours. The coated mica gives a transparent appearance and
soft brilliance to skin.
In antiperspirant or deodorant compositions, it is known to encapsulate or
coat a deodorant active or a fragrance added to the deodorant or
antiperspirant composition however, it is virtually unknown to encapsulate
antiperspirant actives.
U.S. Pat. No. 4,803,195 to Holzner teaches a personal care composition
having deodorant or antiperspirant activity comprising the deodorant or
antiperspirant active and a perfume base wherein the perfume base is
either in the form of an aqueous emulsion or in microencapsulated form.
The perfume is released upon contact with moisture and can be re-
encapsulated in situ.
U.S. Pat. No. 4,818,522 to Ferentchak et al. teaches antiperspirant
compositions comprising water-immiscible adjuvants which are encapsulated
in thick-walled, hallow, substantially spherical particles of an
antiperspirant active. The water immiscible adjuvants include fragrances,
antibacterials, antimicrobial or antifungal agents, deodorants or other
dermatological preparations. The antiperspirant actives are the
encapsulant material therefore Ferentchak et al. does not teach a method
for encapsulating antiperspirant actives. The encapsulated
water-immiscible adjuvants are prepared by emulsifying the adjuvant in an
aqueous solution of the antiperspirant active and spray drying the
resulting material.
EP Patent No. 0303461 to Wright teaches antiperspirant and deodorant
compositions containing moisture sensitive capsules which in the presence
of moisture release sensory agents such as perfumes, skin coolants,
emollients or other benefit agents such as deodorant actives,
antiperspirant actives, and anticholinergic actives. The special polymer
from which the capsules are formed is preferably a polysaccharide. The
method for preparing the capsules comprises preparing an emulsion of
water, the special polymer and the sensory or benefit agent and spray
drying the emulsion. The only benefit obtained through the encapsulation
of the antiperspirant active is believed to be the ability to produce
stable alcoholic compositions and release of the agent in the presence of
moisture.
U.S. Pat. No. 4,524,062 to Laba et al. teaches an antiperspirant/deodorant
stick composition which comprises a powdered antiperspirant active, a
coating material for the antiperspirant active, a deodorant and a cologne
stick base. The coating material is typically a glycol stearate and the
coated antiperspirant active is achieved by blending the antiperspirant
active and the glycol stearate at a temperature at which the glycol
stearate is a liquid. U.S. Pat. No. 4,524,062 does not teach a process for
obtaining the antiperspirant active in an encapsulated form and there is
no evidence to show that the antiperspirant active is even coated and not
merely suspended in the glycol stearate.
It is an object of this invention to show encapsulated aluminum-zirconium
halohydrate compositions.
It is further an object of this invention to show a method for producing
the encapsulated aluminum-zirconium halohydrate compositions.
It is further an object of this invention to show a method for producing
encapsulated aluminum-zirconium halohydrate compositions of a controlled
particle size and shape.
It is further an object of this invention to show deodorant and
antiperspirant compositions comprising the encapsulated aluminum-zirconium
salt.
THE INVENTION
The encapsulated aluminum-zirconium salts of this invention are comprised
of aluminum-zirconium halohydrate contained in a shell comprised of a
carboxylic acid or carboxylic acid derivative (herein referred to as
carboxylate). Upon contact with moisture, the shell opens up and releases
the aluminum-zirconium halohydrate. Some or all of the aluminum-zirconium
halohydrate may be dissolved in the moisture, depending on the
concentration of the salt and the amount of moisture.
The encapsulated aluminum zirconium salts of this invention are produced by
combining together, with agitation, an aqueous aluminum-zirconium
halohydrate salt, a non-water miscible hydrophobic liquid (herein referred
to as hydrophobic liquid), and a carboxylate and heating the mixture to a
temperature sufficient to remove substantially all free water. Some of the
hydrophobic liquid may be removed during the heating because of an
azeotrope that may form between the hydrophobic liquid and the water. It
is important that the rate of water distillation be faster than the rate
of hydrophobic liquid distillation. It is preferred that any azeotrope
formed contain more than 50% by weight of water. After the removal of the
water, the encapsulated aluminum-zirconium salts precipitate out of the
reaction medium. Typically, an increase in the temperature will occur when
the distillation of the aqueous phase is complete. Upon completion of the
distillation there should be enough fluid remaining to keep the
encapsulated aluminum-zirconium salts free flowing. The encapsulated
aluminum-zirconium salts can then recovered through separation means such
as filtration.
The aqueous aluminum-zirconium halohydrates useful in the instant invention
are those currently known in the art. The aluminum-zirconium halohydrates
may be exemplified by aluminum-zirconium chlorohydrate, aluminum-zirconium
bromohydrate, and aluminum-zirconium iodohydrate and mixtures thereof. The
aluminum-zirconium halohydrates are typically buffered with an amino acid
such as glycine. The aluminum-zirconium halohydrates useful in the instant
invention may be further described as a standard (non-activated) or an
activated salt. An activated salt, through compositional differences, is
more efficacious when used in antiperspirant compositions.
The aluminum-zirconium halohydrates useful in the instant invention may be
further described by the formula
Al.sub.a Zr.sub.b (OH).sub.c X.sub.d
where a/b has the value of 0 to 20, b has a value of treater than 0,
3a+4b=c+d; and X is selected from Cl, Br, I and NO.sub.3.
The aluminum-zirconium halohydrate may be supplied as an aqueous solution
containing greater than 0% by weight of the aluminum-zirconium
halohydrate. The maximum amount of aluminum-zirconium halohydrate in the
aqueous solution is dependent upon its solubility in water. Typically the
aluminum-zirconium halohydrate is used as an aqueous solution comprising
10% to 40% by weight of the aluminum-zirconium halohydrate. Aqueous
solutions containing less than 10% by weight of the aluminum-zirconium
halohydrate may be used to produce an encapsulated aluminum-zirconium
salt, however, they are not economically advantageous. Aqueous solutions
containing greater than 40% by weight of the aluminum- zirconium
halohydrate are not well known in the art however, they are useful when
obtainable.
Non-water miscible hydrophobic liquids useful in the instant invention may
be selected from low viscosity silicone fluids, paraffin oils such as
mineral oil, and mixtures thereof. The low viscosity silicones and
further, low viscosity cyclic siloxanes are the preferred hydrophobic
liquid.
Low viscosity silicones useful in the instant invention are selected from
cyclic and linear silicones and mixtures thereof which have a viscosity of
less than 1,000 centistokes. The cyclic low viscosity silicones may be
exemplified by compounds having the formula
##STR1##
wherein each R is independently selected from an alkyl group containing 1
to 30 carbon atoms and an aryl group containing 6 to 10 carbon atoms and x
has the value of 3 to 10. The preferred cyclic low viscosity silicone is
when R is predominantly methyl and x is 4 to 5.
The cyclic low viscosity silicones may be further exemplified by, but not
limited to hexamethylcyclotri- siloxane, octamethylcyclotetrasiloxane,
decamethylcyclo- pentasiloxane, dodecamethylcyclohexasiloxane and mixtures
thereof.
The linear low viscosity silicones may be exemplified by compounds having
the formula
##STR2##
wherein each R is independently selected from an alkyl group containing 1
to 3 carbon atoms and an aryl group containing 6 to 10 carbon atoms: R" is
selected from R and a hydroxyl group (--OH); and y has the value such that
the viscosity of less than 1,000 centistokes. The preferred linear low
viscosity silicone is when R is predominantly methyl.
The linear low viscosity silicones may be further exemplified by, but not
limited to, trimethylendblocked dimethylpolysiloxane fluids. 5, 10. 25 and
50 cS dimethylpolysiloxane fluids, octamethyltrisiloxane,
decamethyltetrasiloxane, hydroxyl endblocked polydimethylsiloxanes, and
mixtures thereof.
The carboxylates useful in the instant invention are selected from the
group consisting of carboxylic acids, alkali metal carboxylates, glyceryl
carboxylates, carboxylic acid anhydrides, carboxylic acid chlorides and
mixtures thereof. The carboxylates useful in the instant invention may be
further exemplified by the formulas:
##STR3##
wherein R.sup.1 is selected from the group consisting of a saturated or
unsaturated, branched or linear alkyl group consisting of at least 2
carbon atoms and a substituted or unsubstituted phenyl group consisting of
at least 6 carbon atoms; and Z is selected from the hydrogen atom, alkali
metals, and glyceryl. R.sup.1 may be further exemplified by, but not
limited to, ethyl, propyl, octyl, decyl, undecyl, pentadecyl, hexadecyl,
octadecyl, doeicosyl, phenyl, phenyl ethylene, and others. Z may be
further exemplified by, but not limited to, the hydrogen atom, sodium,
potassium, --CH.sub.2 CH(OH)CH.sub.2 OH, and --CH(OH)CH.sub.2 OH.
For the carboxylates to be useful in the instant invention it is necessary
for the carboxylate to be soluble in the hydrophobic liquid and/or to have
a melting point less than the water distillation temperature and further,
the carboxylate must not be completely distillable at the water
distillation temperature. When using a carboxylate where Z is an alkali
metal it may be necessary to add a co-solvent, such as water, to
completely dissolve the alkali metal carboxylate.
The carboxylates useful in the instant invention may be further exemplified
by, but are not limited to, butyric acid, caprylic acid, lauric acid,
palmitic acid, stearic acid, isostearic acid, behenic acid, oleic acid,
linoleic acid, linolenic acid, phenylacetic acid, sodium stearate, sodium
palmitate, potassium stearate, glyceryl monostearate, stearic anhydride,
palmitic anhydride, lauric anhydride, stearoyl chloride, myristyoyl
chloride, octanoyl chloride and mixtures thereof. The preferred
carboxylate is stearic acid due to it being a cosmetically acceptable
ingredient and it has the acceptable properties to make it useful.
The encapsulated aluminum-zirconium salts are formed by combining at least
14 millimoles of carboxylate for every 100 parts of aluminum-zirconium
halohydrate solids, and at least 1 part of hydrophobic liquid for every
part of water. It is preferred to use between 35 to 200 millimoles of
carboxylate per every 100 parts of aluminum-zirconium halohydrate solids
and at least 1.25 parts hydrophobic liquid per every part of water. It may
be possible to use less than one part of hydrophobic liquid for every part
of water if the amount of hydrophobic liquid lost in the distillation
azeotrope is replaced during the encapsulation.
The aqueous aluminum-zirconium halohydrate, carboxylate and hydrophobic
liquid are combined and heated, with agitation, to a temperature
sufficient to remove substantially all of the free water from the solution
(water distillation temperature). Typically temperatures greater than
100.degree. C., preferably 100.degree. to 130.degree. C., at atmospheric
pressure are useful for removing any water. When the water has been
removed the temperature will rise above the water distillation
temperature. It is preferred that the temperature does not exceed
150.degree. C. for an extended period of time. Temperatures which exceed
150.degree. C. for an extended period of time may be detrimental to the
encapsulant and lead to fragmentation or cracking of the shell and
possibly the conversion of the aluminum-zirconium halohydrate into an
aluminum-zirconium oxide. Pressures greater or less than atmospheric
pressure can be employed in the method of the instant invention thereby
allowing the mixture to be heated to higher or lower temperatures for the
removal of the water. It is essential that the water be removed during the
heating step. Merely heating to temperatures greater than 100.degree. C.
while refluxing, or containing the water otherwise, will not result in an
encapsulated aluminum-zirconium salt. Typically, the completion of the
water removal will be indicated by an increase in the temperature above
the water distillation temperature.
After the removal of the water from the mixture, the encapsulated
aluminum-zirconium salts precipitate out of the reaction medium. The
encapsulated aluminum zirconium salts are typically recovered from the
reaction medium by filtration means such as gravimetric, pressure or
vacuum filters or by other separation means such as decanting or
centrifuging. Filtration means will vary depending on the batch size. It
is preferred to recover the encapsulated aluminum-zirconium salts from the
reaction medium at a temperature at or above the temperature at which the
carboxylate is a liquid. It is further preferred to recover the
encapsulated aluminum-zirconium salts from the reaction medium using
filtration means.
After the encapsulated aluminum-zirconium salts have been recovered by
filtration means from the reaction medium, they may be optionally washed
using a hydrophobic solvent to remove any excess carboxylate that might be
adhered to the shells. If the carboxylate is not a liquid at room
temperature it may be necessary to heat the hydrophobic liquid to a
temperature at which the carboxylate is a liquid during the wash.
It is theorized that the shell material of the encapsulated
aluminum-zirconium salt is comprised of mostly carboxylate, however, it
may contain some hydrophobic liquid which may have been entrapped within
the coating. Further, it is theorized that the shell comprises less than
5% and more likely less than 1% of the total encapsulated aluminum-
zirconium salt mass. It is further theorized that the coating thickness is
dependent upon the concentration of the carboxylate used. Typically the
shells are spherical in nature however, they may also be elliptical,
elongated or shaped otherwise. The standard aluminum-zirconium halohydrate
salts do not appear to undergo a compositional change during the
encapsulation process based on High Performance Liquid Chromatography
(HPLC).
The aluminum-zirconium halohydrates do not appear to be released from
within the shell in any solvent or liquid except water or solvents
containing water. In the presence of water the shells open up releasing
the aluminum-zirconium salt and some or all of the aluminum-zirconium salt
may be dissolved in the water depending on the amount of water present.
Certain solvents such as paraffin oil, toluene, ethanol, hexanes,
propylene glycol, isopropyl myristate, and silicone glycol copolymers, did
not appear to affect the shell or release the salt.
Another aspect of this invention is the ability to produce encapsulated
aluminum-zirconium salts having a controlled particle size and shape. This
aspect is accomplished by control of the concentration of the carboxylate
and control of the agitation rate. The encapsulated aluminum-zirconium
salts of this invention are produced using 15 or more millimoles of
carboxylate per every 100 parts aluminum-zirconium halohydrate solids. As
the amount of carboxylate used increases, the beads formed become more
spherical in shape and uniform in size. Thus, the use of higher amounts of
carboxylate may result in uniform, spherical beads.
Particle size distribution is controlled by the agitation rate (the rate of
agitation during the water distillation). Encapsulated aluminum-zirconium
salts which resemble impalpable powder (5 to 75 microns) can be produced
at higher agitation rates. Because of equipment differences, mixing
characteristics and other factors, it is not possible to specify an exact
agitation rate that will produce an exact particle size however, one
skilled in the art would be able to determine this for a specific
apparatus.
The encapsulated aluminum-zirconium salts of the instant invention are
useful in deodorant and antiperspirant compositions such as aerosols,
roll-ons, and sticks. It is preferable for the deodorant and
antiperspirant compositions to be anhydrous, however, it is not necessary.
The aerosol compositions are typically comprised of 1 to 20% by weight,
preferably 8 to 12 wt. %, of an encapsulated aluminum-zirconium salt; 50
to 90% by weight of a propellant, such as butane, isobutane, propane,
nitrogen, carbon dioxide; and 5 to 15% by weight of an anhydrous carrier
such as cyclomethicone and ethanol. Optional ingredients, such as
cyclomethicone, dimethicone, isopropyl myristate, isopropyl palmitate,
fragrance, valve lubricants, talc, silica, suspending aids, polar
activators, deodorants and others may be added into the aerosol
compositions to improve the aesthetics or to change the characteristics of
the propulsion. The aerosol compositions are produced using methods known
in the art.
The roll-on compositions are typically comprised of 1 to 20% by weight,
preferably 10 to 25 wt. % of an encapsulated aluminum-zirconium salt; 60
to 95% by weight of a carrier liquid, such as water, cyclomethicone,
organic esters and derivatives of organic esters, dioctyl adipate and
others; and optionally 0.1 to 5% by weight of a suspending aid or 0.1 to
10% by weight of an emulsifier, such as glycerol monostearate, steareth-2,
alkoxylates and others. If a suspending aid is used 0.1 to 2% of a polar
activator must also be added. Other optional ingredients, such as
fragrance, deodorants, talc, silica, polyethylene, silica, dimethicone,
aluminum sulfate, starch, octenyl succinate and others, may be added into
the roll-on compositions to improve the aesthetics or increase the
viscosity of the composition. The roll-on compositions are produced using
methods known in the art.
The stick compositions are typically comprised of 1 to 20% by weight,
preferably 15 to 25 wt. % of an encapsulated aluminum-zirconium salt; 20
to 65% by weight of a carrier fluid such as cyclomethicone, ethanol or
propylene glycol; and 5 to 30% by weight of a gellant such as cetyl
alcohol, stearyl alcohol, or hydrogenated caster oil. Optional
ingredients, such as organic esters, organic ethers, dimethicone,
emulsifiers, talc, silica, fragrance, deodorant, polyethylene and others,
may be added to the stick compositions to improve the aesthetics or
application of the encapsulated aluminum zirconium salt. The stick
compositions are produced using methods known in the art.
Deodorant and antiperspirant compositions such as pump sprays, creams,
lotions and others may also formulated with the encapsulated
aluminum-zirconium salts.
So that those skilled in the art can understand and appreciate the
invention taught herein, the following examples are presented, it being
understood that these examples should not be used to limit the scope of
this invention over the limitation found in the claims attached hereto.
The term "parts" employed herein refers to parts by weight.
Particle Size Analysis: The particle size of the encapsulated
aluminum-zirconium salts was determined by using a Malvern 3600 EZ
particle sizer. For analysis, the encapsulated salts were suspended in a
solvent selected from cyclomethicone or toluene and the stir speed was set
at 4.
Physical Characteristics: The physical characteristics of the encapsulated
aluminum-zirconium salts (shape, cracks, jagged edges, etc.) was
determined by observing the encapsulated aluminum-zirconium salts under a
40.times. microscope.
Some of the encapsulated and unencapsulated aluminum-zirconium salts were
analyzed by HPLC according to the method taught in European Patent
Application 0 256 831, herein incorporated by reference. Sample
preparation for the encapsulated aluminum-zirconium salts comprises
weighing 1.0 gram of the encapsulated aluminum-zirconium salt into a vial
and adding 0.01N HCl to the vial until the total sample weight is 10
grams. The sample is shaken. 2 to 3 ml of the liquid are drawn off and
filtered through a 0.45 micron syringe filter. The injected sample size is
2.0 microliters. In the instant application, Peak 4 corresponds with Band
III, Peak 3 corresponds with Band 11 and Peak 2 corresponds with Band I as
defined in European Patent Application 0 256 831.
EXAMPLE 1
300 grams of a mixture comprised of octamethylcyclotetrasiloxane and
decamethylcyclopentasiloxane and 9.9 grams of stearic acid were combined
in a 1 liter beaker and heated to 80.degree. C. 300 grams of aqueous
Aluminum-Zirconium Tetrachlorohydrex-Gly (35% solids) was added to the
stearic acid solution, with agitation. The mixture was heated for
approximately 1 hour, while evaporating off the water, maintaining a
temperature around 100.degree. C. The reaction was stopped when the pot
temperature reached approximately 110.degree. C. and no more water was
observed to be evaporating off. The mixture was then vacuum filtered
(while hot, .about.112.degree. C.). using a Buchner funnel, to recover the
encapsulated aluminum- zirconium salt.
The encapsulated aluminum-zirconium salt appeared to be spherical and were
white in color.
EXAMPLE 2
300 grams of a mixture comprised of octamethylcyclotetrasiloxane and
decamethylcyclopentasiloxane and 11.88 grams of stearic acid were combined
in a 1L round bottom flask equipped with a paddle-blade agitator, a water
cooled condenser and a 1 L round bottom receiver and heated to 67.degree.
C. 300 grams of aqueous Aluminum-Zirconium Tetrachlorhydrex-Gly (35%
solids), heated to 70.degree. C., was added to the stearic acid solution,
with agitation. The mixture was heated for approximately 2.25 hours, while
distilling off the water, maintaining a temperature around 110.degree. C.
The reaction was stopped when the pot temperature reached approximately
122.degree. C. and no more water was observed to be distilling off. The
mixture was then vacuum filtered (while hot, .about.122.degree. C.), using
a Buchner funnel, to recover 108.6 grams of the encapsulated
aluminum-zirconium salt. The beads were re-dispersed in 100 grams of a
mixture comprised of octamethylcyclotetrasiloxane and
decamethylcyclopentasiloxane and heated to 70.degree. C. and filtered
again. 104.1 grams of encapsulated aluminum- zirconium salt was recovered
after the second filtration.
The encapsulated aluminum-zirconium salts were mostly spheres of varying
sizes.
EXAMPLE 3
300 grams of a mixture comprised of octamethylcyclotetrasiloxane and
decamethylcyclopentasiloxane and 13.86 grams of stearic acid were combined
in a 1 L beaker and heated to 70.degree. C. 300 grams of aqueous
Aluminum-Zirconium Tetrachlorhydrex-Gly (35% solids) was added to the
stearic acid solution, with agitation. The mixture was heated for
approximately 2 hours, while evaporating off the water, maintaining a
temperature around 100.degree. C. The reaction was stopped when the pot
temperature reached approximately 112.degree. C. and no more water was
observed to be evaporating off. The mixture was then vacuum filtered
(while hot, .about.112.degree. C.), using a Buchner funnel to recover the
encapsulated aluminum-zirconium salts.
EXAMPLE 4
150 grams of a mixture comprised of octamethylcyclotetrasiloxane and
decamethylcyclopentasiloxane and 6.3 grams of caprylic acid were combined
in a 500 ml round bottom flask equipped with a paddle-blade agitator, a
water cooled condenser an a 250 ml round bottom receiver. 150 grams of
aqueous Aluminum-Zirconium Tetrachlorhydrex-Gly (35% solids) was added to
the caprylic acid solution, with agitation. The mixture was heated for
approximately 4 hours, while distilling off the water, maintaining a
temperature around 110.degree. C. The reaction was stopped when the pot
temperature reached approximately 130.degree. C. and no more water was
observed to be distilling off. The mixture was cooled and vacuum filtered
using a Buchner funnel, to recover the encapsulated aluminum-zirconium
salt.
EXAMPLE 5
150 grams of a mixture comprised of octamethylcyclotetrasiloxane and
decamethylcyclopentasiloxane and 6.3 grams of iso-stearic acid were
combined in a 500 ml round bottom flask equipped with a paddle-blade
agitator, a water cooled condenser an a 250 ml round bottom receiver. 150
grams of aqueous Aluminum-Zirconium Tetrachlorhydrex-Gly (35% solids) was
added to the iso-stearic acid solution, with agitation. The mixture was
heated for approximately 4 hours, while distilling off the water,
maintaining a temperature around 107.degree. C. The reaction was stopped
when the pot temperature reached approximately 127.degree. C. and no more
water was observed to be distilling off. The mixture was vacuum filtered
(.about.80.degree. C.) using a Buchner the encapsulated aluminum-
zirconium salt.
The encapsulated aluminum-zirconium salts were uniform in size and mostly
spherical.
EXAMPLE 6
150 grams of a mixture comprised of octamethylcyclotetrasiloxane and
decamethylcyclopentasiloxane and 6.3 grams of behenic acid were combined
in a 500 ml round bottom flask equipped with a paddle-blade agitator, a
water cooled condenser an a 250 ml round bottom receiver and heated to
approximately 75.degree. C. 150 grams of aqueous Aluminum-Zirconium
Tetrachlorhydrex-Gly (35% solids) was added to the behenic acid solution,
with agitation. The mixture was heated for approximately 4.5 hours, while
distilling off the water, maintaining a temperature around 102.degree. C.
The reaction was stopped when the pot temperature reached approximately
135.degree. C. and no more water was observed to be distilling off. The
mixture was vacuum filtered (.about.135.degree.) using a Buchner funnel,
to recover the encapsulated aluminum-zirconium salt. The particles were
mostly spherical and yellow.
EXAMPLE 7
150 grams of a mixture comprised of octamethylcyclotetrasiloxane and
decamethylcyclopentasiloxane and 6.3 grams of glyceryl monostearate were
combined in a 500 ml round bottom flask equipped with a paddle-blade
agitator, a water cooled condenser and a 250 ml round bottom receiver and
heated to approximately 70.degree. C. 150 grams of aqueous
Aluminum-Zirconium Tetrachlorhydrex-Gly (35% solids) was added to the
glyceryl monostearate solution, with agitation. The mixture was heated for
approximately 3.5 hours, while distilling off the water, maintaining a
temperature around 100.degree. C. The reaction was stopped when the pot
temperature reached approximately 130.degree. C. and no more water was
observed to be distilling off. The mixture was vacuum filtered
(.about.85.degree.) using a Buchner funnel, to recover the encapsulated
aluminum- zirconium salt. The particles were mostly spherical.
EXAMPLE 8
150 grams of a mixture comprised of octamethylcyclotetrasiloxane and
decamethylcyclopentasiloxane and 6.3 grams of sodium stearate were
combined in a 500 ml round bottom flask equipped with a paddle-blade
agitator, a water cooled condenser an a 250 ml round bottom receiver and
heated to approximately 90.degree. C. 100 grams of deionized water was
added to dissolve the sodium stearate. 150 grams of aqueous
Aluminum-Zirconium Tetrachlorhydrex-Gly (35% solids) was added to the
sodium stearate solution, with agitation. The mixture was heated for
approximately 3.5 hours, while distilling off the water, maintaining a
temperature around 105.degree. C. The reaction was stopped when the pot
temperature reached approximately 135.degree. C. and no more water was
observed to be distilling off. The mixture was vacuum filtered
(.about.99.degree.) using a Buchner funnel, to recover the encapsulated
aluminum- zirconium salt.
EXAMPLE 9
300 grams of a polydimethylsiloxane fluid having a viscosity of 50
centistokes and 11.8 grams of stearic acid were combined in a 1 L round
bottom flask equipped with a paddle-blade agitator, a water cooled
condenser and a 250 ml round bottom receiver and heated to approximately
70.degree. C. 300 grams of aqueous Aluminum-Zirconium Tetrachlorhydrex-Gly
(35% solids) was added to the stearic acid solution, with agitation. The
mixture was heated for approximately 1.5 hours, while distilling off the
water, maintaining a temperature around 100.degree. C. The reaction was
stopped when no more water was observed to be distilling off. The mixture
was vacuum filtered (.about.80.degree.) using a Buchner funnel, to recover
the encapsulated aluminum-zirconium salt. The particles were yellow.
EXAMPLE 10
150 grams of a polydimethylsiloxane fluid having a viscosity of 10
centistokes and 6.3 grams of stearic acid were combined in a 500 ml round
bottom flask equipped with a paddle-blade agitator, a water cooled
condenser an a 250 ml round bottom receiver and heated to approximately
75.degree. C. 150 grams of aqueous Aluminum-Zirconium Tetrachlorhydrex-Gly
(35% solids) was added to the stearic acid solution, with agitation. The
mixture was heated for approximately 3 hours, while distilling off the
water, maintaining a temperature around 115.degree. C. The reaction was
stopped when the pot temperature reached approximately 135.degree. C. and
no more water was observed to be distilling off. The mixture was vacuum
filtered (.about.80.degree. C.) using a Buchner funnel, to recover the
encapsulated aluminum-zirconium salt.
EXAMPLE 11
150 grams of a mixture comprised of octamethylcyclotetrasiloxane and
decamethylcyclopentasiloxane (cyclomethicone) and 6.3 grams of stearic
anhydride were combined in a 500 ml round bottom flask equipped with a
paddle-blade agitator, a water cooled condenser and a 250 ml round bottom
receiver. The mixture was heated to 85.degree. C. 150 grams of aqueous
Aluminum-Zirconium Tetrachlorhydrex-Gly (35% solids) was added to the
stearic anhydride solution, with agitation. The mixture was heated for
approximately 1.5 hours, while distilling off the water, maintaining a
temperature around 106.degree. C. The reaction was stopped when the pot
temperature reached approximately 127.degree. C. The mixture was vacuum
filtered (.about.85.degree. C.) using a Buchner funnel, to recover 50.07
grams encapsulated aluminum-zirconium salt.
EXAMPLE 12
150 grams of a mixture comprised of octamethylcyclotetrasiloxane and
decamethylcyclopentasiloxane and 6.6 grams of stearoyl chloride were
combined in a 500 ml round bottom flask equipped with a paddle-blade
agitator, a water cooled condenser and a 250 ml round bottom receiver. The
mixture was heated to 85.degree. C. 150 grams of aqueous
Aluminum-Zirconium Tetrachlorhydrex-Gly (35% solids) was added to the
stearoyl chloride acid solution, with agitation. The mixture was heated
for approximately 2 hours, while distilling off the water, maintaining a
temperature around 105.degree. C. The reaction was stopped when the pot
temperature reached approximately 130.degree. C. The mixture was vacuum
filtered (85.degree. C.) using a Buchner funnel, to recover 57.34 grams of
encapsulated aluminum-zirconium salt.
EXAMPLE 13
Four experiments were conducted to determine the effect of agitation rate
on particle size. In the experiments 150 grams of a mixture comprised of
octamethylcyclotetrasiloxane and decamethylcyclopentasiloxane and 6.3
grams of stearic acid were combined in a 500 ml round bottom flask
equipped with a paddle-blade agitator, a water cooled condenser and a 250
ml round bottom receiver and heated to 75.degree. C. 150 grams of aqueous
Aluminum-Zirconium Tetrachlorhydrex-Gly (35% solids), was added to the
stearic acid solution, with agitation. The mixture was heated while
distilling off the water. The agitation during the distillation was
maintained at various levels given in Table 1. The reaction was stopped
when there was no more water observed to be distilling off. The mixture
was then vacuum filtered using a Buchner funnel, to recover the
encapsulated aluminum-zirconium salt. The particle size of the resulting
encapsulated aluminum-zirconium salts was measured using a Malvern 3600 EZ
particle sizer. Results are given in Table 1.
TABLE 1
______________________________________
Agitation Particle Size
(microns)
Speed Distribution
Average
______________________________________
150 113 to 262 199
200 125 to 270 199
400 25 to 270 130
650 7 to 65 27
______________________________________
EXAMPLE 14
An suspension stick composition was produced by heating 55 parts of
cyclomethicone and 20 parts of stearyl alcohol to 65.degree. C. with
stirring. 2 parts of PPG-14 Butyl Ether was then added with continued
stirring followed by 1 part of hydrogenated caster oil, 2 parts of talc
and 20 parts of an encapsulated aluminum-zirconium salt produced as in
Example 1. The mixture was cooled to 53.degree. C. and cast into a stick.
EXAMPLE 15
An aerosol composition was produced by mixing 12 parts of an encapsulated
aluminum-zirconium salt as produced in Example 1 with 10.5 parts of
cyclomethicone and 2 parts of dimethicone. This mixture was loaded into an
aerosol container and charged with 75.5 parts of propellant.
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